Dichloromethane → HCID 131733089、化合物

HRID 1518998ノート

反応式

HRID 1518998 の反応式
Cl[C:2]1[CH:13]=[CH:12][C:5]([C:6]([NH:8][CH:9]([CH3:11])[CH3:10])=[O:7])=[C:4]([NH:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:3]=1.C(N(C(C)C)CC)(C)C.[CH3:31][N:32]1[C:36]([S:37](Cl)(=[O:39])=[O:38])=[CH:35][CH:34]=[N:33]1.[Cl:41]CCl>O>[Cl:41][C:19]1[CH:20]=[CH:21][C:16]([CH2:15][N:14]([C:4]2[CH:3]=[CH:2][CH:13]=[CH:12][C:5]=2[C:6]([NH:8][CH:9]([CH3:11])[CH3:10])=[O:7])[S:37]([C:36]2[N:32]([CH3:31])[N:33]=[CH:34][CH:35]=2)(=[O:39])=[O:38])=[CH:17][CH:18]=1

参加物

6

反応物 4

HCID 6344Dichloromethane2 回HCID 81531DiisopropylethylamineHCID 224726211-Methyl-1H-pyrazole-5-sulfonyl chlorideHCID 131733090HCID 131733090、化合物

生成物 1

HCID 131733089HCID 131733089、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-(4-Chloro-benzylamino-N-isopropyl-benzamide (30 mg, 0.1 mmol), diisopropylethylamine (35 μL, 0.2 mmol) and 1-methyl-1H-pyrazole-5-sulfonyl chloride (36 mg, 0.2 mmol) were stirred in dry dichloromethane (2 ml) at room temperature for 72 hrs. The reaction was diluted with dichloromethane (5 ml) and water (5 ml) with stirring. The organics were collected, dried (PTFE frit) and concentrated in vacuo. The residue was purified by preparative TLC (10% ethyl acetate/dichloromethane) to yield the product as an off-white solid (11.9 mg). HPLC retention time 8.04 min. Mass spectrum (ES+) m/z 44 (M+H).

後処理

  1. customThe organics were collected
  2. dry with materialdried (PTFE frit)
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by preparative TLC (10% ethyl acetate/dichloromethane)

出典と根拠

ORDレコード
ord-b3110d3a783e46479a3502e47ca751a4
出典データセット
uspto-grants-2015_07
特許番号
US09073834B2

反応ノート

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